2D nanomaterials are emerging rapidly because of their exceptional chemical and physical properties. Reducing the thickness or number of crystalline layers improves the catalytic performance of many semiconductors, and thus, different exfoliation strategies have been proposed. However, many exfoliation methods can cause damage or chemical modifications, and control over size and aggregation can be problematic. Herein, In_(2)S_(3) was grown in the surfactant-modified interlayer space of the layered silicate clay Laponite, leading to a hybrid nanostructure containing 1–1.5 nm thick lamellae of In_(2)S_(3). The synthetic parameters varied the thickness and regularity of the In_(2)S_(3) layers, and drastic changes in photophysical properties were observed, underlining the importance of colloidal interactions for templated growth. Photocurrent measurements and photocatalysis experiments showed that more than an order of magnitude increased apparent quantum efficiency and internal photon to current conversion efficiency over In_(2)S_(3). This was attributed to fast interfacial charge transfer, enhanced redox capability, and improved charge transport properties of the In_(2)S_(3) layers because of reduced layer thickness and isolation by magnesiosilicate nanoclay in between. Overall, this study provides a simple colloidal approach to grow defined layered heterostructures of In_(2)S_(3) with limited thickness and enhanced photophysical properties, allowing improved catalysis. The photocatalytic enhancement, facile synthesis, and increased product yield compared with pure In_(2)S_(3) make these promising materials for energy conversion and environmental remediation.
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